CN114561544A - Application of lithium carbonate seed crystal in recovering lithium in battery by hydrometallurgy - Google Patents
Application of lithium carbonate seed crystal in recovering lithium in battery by hydrometallurgy Download PDFInfo
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- CN114561544A CN114561544A CN202210246858.0A CN202210246858A CN114561544A CN 114561544 A CN114561544 A CN 114561544A CN 202210246858 A CN202210246858 A CN 202210246858A CN 114561544 A CN114561544 A CN 114561544A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
The invention discloses an application of lithium carbonate seed crystals in the hydrometallurgical recovery of lithium in batteries, which comprises the following specific implementation processes: adding a certain amount of sodium carbonate into lithium-containing waste liquid of a lithium battery recovered through hydrometallurgy, gradually adding a sodium hydroxide solution or a hydrochloric acid solution to adjust the pH value of the waste liquid to 11.0 +/-0.2, adding a certain amount of lithium carbonate seed crystal into the waste liquid after the pH is adjusted, inducing nucleation and growth of lithium carbonate crystals in a water bath at 25-50 ℃, removing a supernatant after 12.5-40 hours, adding ethanol to wash a bottom precipitate, centrifugally collecting a precipitate product, performing vacuum drying, and finally recovering the lithium carbonate product to achieve the purpose of recovering lithium in the lithium-containing waste liquid. Compared with the traditional lithium extraction and recovery process, the method has mild and green implementation conditions, high recovery efficiency, simple operation and convenient industrialization.
Description
Technical Field
The invention belongs to the technical field of lithium recovery, and particularly relates to application of lithium carbonate seed crystals in recovery of lithium in batteries by hydrometallurgy.
Background
The recovery process of Lithium Ion Batteries (LIBs) can be classified into a dry metallurgy recovery process, a biological recovery process and a wet metallurgy recovery process according to the difference of the recovery processes. Relatively speaking, wetThe method has the advantages of mature recovery process, high commercialization degree and wide application range. The method mainly utilizes a proper chemical reagent to selectively separate out metal elements in the solution, thereby achieving the purpose of recovery. At present, although the wet recovery process using sulfuric acid as a leaching agent can realize effective separation of metal elements such as cobalt, nickel, copper and iron, the recovery efficiency of lithium element is still very low, lithium ion concentration is low, and lithium ion cannot be effectively converted into a difficult-to-dissolve salt of lithium carbonate serving as a battery raw material, and a common high-temperature evaporation step is adopted
So that the precipitation energy consumption is large, the recovery cost is high, and the development of lithium resource recovery is restricted. Therefore, the technology for recovering lithium in the waste lithium battery by improving hydrometallurgy is improved, the low cost of lithium resources is realized, and the efficient extraction and recovery become very important under the mild condition.
CN106848473A discloses a selective recovery method of lithium in waste lithium iron phosphate batteries, which comprises the steps of firstly selecting a conventional high-temperature roasting separation process to recover aluminum, then obtaining impurities containing iron and lithium by ball milling treatment, and then adding H2O2、MnO2、KMnO4The whole process flow is complex, the oxidizing agent, the alkali liquor and the precipitating agent need to be added for many times, and the first step of the process needs to be continuously heated at a high temperature of more than 400 ℃ to keep the normal operation of the roasting separation process, thereby causing extremely high energy consumption and serious secondary pollution. On the other hand, in the lithium recovery process, due to the addition of the early oxidant and the precipitant, the concentration of lithium ions in the solution is continuously reduced, a large amount of saturated sodium carbonate solution needs to be added, and the solvent is heated and evaporated to precipitate lithium carbonate to recover lithium, so that high recovery cost is caused.
CN113415814A provides a method for selectively recovering lithium from waste lithium ion batteries by ultra-low temperature roasting aiming at the problems of high energy consumption and environment caused by a high temperature roasting and sorting process, but the temperature of ultra-low temperature roasting and sorting in the process still needs 300 ℃, although the temperature is reduced compared with the temperature of the conventional high temperature roasting and sorting process, the continuous heating process still causes higher energy consumption and causes environmental pollution; meanwhile, the powder subjected to ultralow temperature roasting and sorting needs to be sieved by a 200-400-mesh sieve, so that the complexity of the whole process is increased undoubtedly, a large amount of saturated sodium carbonate solution still needs to be added for lithium recovery in the process, the solvent is heated and evaporated to precipitate lithium carbonate for lithium recovery, and the recovery cost is still high.
CN108550939A discloses a method for selectively recovering lithium from waste lithium batteries and preparing lithium carbonate, which comprises the steps of nitrifying a positive electrode material in the waste lithium batteries in order to further reduce the roasting separation temperature, converting valuable metals in the positive electrode material into nitrates through a nitration reaction, roasting the nitrates to obtain calcines, leaching the calcines for multiple times, filtering to obtain a lithium-rich solution, adding carbonates into the lithium-rich solution, and performing reaction and precipitation to obtain lithium carbonate; although the roasting separation temperature is reduced to 200 ℃ by introducing the nitration reaction, the nitration reaction also needs the reaction temperature of 150 ℃, and the addition of the nitration reagent also introduces dangerous factors for industrialization and brings environmental pollution. Secondly, in the process of leaching the calcine for multiple times, although a lithium-rich solution is prepared, the process is complicated and is not beneficial to industrialization, the leaching agent cannot be recycled, and the recycling cost of the whole process is high.
CN102408119A discloses a method for recovering lithium resources by preparing lithium carbonate through crystallization by elution reaction, wherein the main recovery process is to introduce one or more organic reagents selected from methanol, ethanol, propanol, butanol and acetone into a lithium-containing waste liquid system as a reaction elution agent, and then add a carbonate system or carbon dioxide to generate lithium carbonate precipitate, thereby achieving the purpose of recovering lithium carbonate. Although the method is simple to operate, the selected alcohol or ketone leaching agents such as ethanol and the like have the characteristics of inflammability and volatility, and are very easy to bring about the problems of danger and environmental pollution. In addition, the organic elution is difficult to recycle, which causes environmental pollution and high recycling cost.
Therefore, the development of an efficient, green and low-cost lithium resource recovery method is an urgent problem to be solved in the research of a hydrometallurgy recovery process.
Disclosure of Invention
In order to solve the problems, the invention aims to provide an application of lithium carbonate seed crystals in a hydrometallurgical recovery battery.
In order to achieve the purpose, the following technical scheme is provided:
the application of the lithium carbonate seed crystal in the hydrometallurgical recovery of lithium in the battery comprises the following specific implementation processes: adding a certain amount of sodium carbonate into lithium-containing waste liquid of a lithium battery recovered through hydrometallurgy, gradually adding a sodium hydroxide solution or a hydrochloric acid solution to adjust the pH value of the waste liquid to 11.0 +/-0.2, adding a certain amount of lithium carbonate seed crystal into the waste liquid after the pH is adjusted, inducing nucleation and growth of lithium carbonate crystals in a water bath at 25-50 ℃, removing a supernatant after 12.5-40 hours, adding ethanol to wash a bottom precipitate, centrifugally collecting a precipitate product, performing vacuum drying, and finally recovering the lithium carbonate product to achieve the purpose of recovering lithium in the lithium-containing waste liquid.
Furthermore, the concentration of lithium sulfate in the lithium-containing waste liquid of the lithium battery is 0.02-0.4 mol/L, and the volume ratio of the molar input amount of sodium carbonate to the lithium-containing waste liquid of the lithium battery is 0.02-0.4 mol/L.
Furthermore, the concentration of the sodium hydroxide solution or the hydrochloric acid solution is 0.01-3 mol/L.
Furthermore, the volume ratio of the molar input amount of the lithium carbonate seed crystal to the lithium-containing waste liquid of the lithium battery is 0.0001-0.0005 mol/L.
Furthermore, the lithium carbonate crystal with the diameter distribution range of 190 nm-6 μm has the crystallinity of 20-100%.
Further, the nucleation and growth time of the crystal seed for inducing the lithium carbonate crystal is 12.5-24 hours.
And further, adding ethanol to wash the sediment at the bottom, centrifuging to obtain a sediment product, and drying the sediment product in a vacuum drying oven at the temperature of 20-100 ℃ for 12-24 hours.
Compared with the prior art, the invention has the beneficial effects that: traditional hydrometallurgy processExtraction step of process lithium
In the method, because the lithium concentration is low, a large amount of precipitator is generally required to be added, and a high-temperature (more than or equal to 400 ℃) evaporation solvent is matched to achieve the purposes of separating out a lithium-containing solute and enriching and recovering lithium, the process has serious secondary pollution and high recovery cost, the application of the lithium carbonate seed crystal in the hydrometallurgical recovery of lithium in the battery can be implemented under the conditions of mild lithium concentration (0.02-0.4 mol/L) without causing secondary pollution and wide range lithium concentration (0.02-0.4 mol/L) only by adding a small amount of seed crystal, and the recovered product lithium carbonate can be directly applied to the aspects of battery manufacturing, medical production, electromagnetic product production and the like.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of lithium carbonate seeds of different sizes;
FIG. 2 is a graph of lithium ion concentration changes detected by inductively coupled plasma emission spectrometer for lithium carbonate seed crystal addition groups of different sizes;
fig. 3 is an SEM image of the products from different size lithium carbonate seed crystal addition sets;
fig. 4 is an X-ray diffraction (XRD) pattern of lithium carbonate seeds of different crystallinity;
fig. 5 is an SEM image of lithium carbonate seeds of different crystallinity;
FIG. 6 is a diagram of lithium ion concentration changes detected by inductively coupled plasma emission spectrometer for lithium carbonate seed crystal adding groups with different crystallinity;
fig. 7 is an SEM image of the products obtained from the lithium carbonate seed crystal addition group of different crystallinity.
Detailed Description
The invention will be further described with reference to the drawings and examples in the following description, but the scope of the invention is not limited thereto.
Preparing lithium carbonate crystal seeds with the same crystallinity and different sizes
The lithium carbonate seed crystal A is purchased from Shanghai Aladdin chemical reagent company, the particle size distribution range is 5.92 +/-1.37 mu m, and the appearance is shown as A in figure 1.
Example 1
Grinding the lithium carbonate seed crystal A by a planetary ball mill to obtain a nano seed crystal B: and continuously grinding 0.5g of lithium carbonate seed crystal A for 30 minutes at the frequency of 30Hz by adopting 2 quartz pots and 8 quartz spheres to obtain the lithium carbonate nano seed crystal B, wherein the particle size distribution range is 580.51 +/-176.93 nm, and the appearance is shown as B in the figure 1.
Example 2
The preparation method of the nano seed crystal C by adopting a dissolution reaction crystallization method comprises the following steps: 400mM Na in 100mL2CO3And 400mM Li2SO450mL of ethanol is added into the mixed solution to serve as an anti-solvent to prepare the lithium carbonate nano seed crystal C, the pH value of the system is adjusted to be 11, the crystallization product of the elution reaction is the required lithium carbonate nano seed crystal C, the particle size distribution range is 317.40 +/-47.14 nm, and the appearance is shown as C in figure 1.
Example 3
The preparation method comprises the following steps of (1) preparing a nano seed crystal D by a solventing-out reaction crystallization method: 400mM Na in 100mL2CO3And 400mM Li2SO450mL of dimethyl sulfoxide (DMSO) is added into the mixed solution to serve as an anti-solvent to prepare lithium carbonate nano seed crystals D, when the pH value of the system is adjusted to be 11, the crystallization product of the elution reaction is the required lithium carbonate nano seed crystals D, the particle size distribution range is 189.52 +/-46.46 nm, and the appearance is shown as D in figure 1.
Example 4
Adding sodium carbonate into lithium battery waste liquid with the concentration of 0.4mol/L of lithium sulfate recovered by hydrometallurgy, wherein the volume ratio of the molar input amount of the sodium carbonate to the lithium-containing waste liquid of the lithium battery is 0.4mol/L, gradually adding 3mol/L of sodium hydroxide solution, adjusting the pH value to 11.0 +/-0.2, dividing the waste liquid with the adjusted pH value into 4 equal parts, respectively adding lithium carbonate seed crystal A and lithium carbonate seed crystal B, C, D prepared in examples 1-3 into the adjusted waste liquid, wherein the volume ratio of the molar input amount of the added lithium carbonate seed crystal to the lithium-containing waste liquid of the lithium battery is 0.0005mol/L, and inducing the nucleation and growth of lithium carbonate crystals in water bath at 50 ℃.
Comparative example 1
Adding sodium carbonate into lithium battery waste liquid with the concentration of 0.4mol/L of lithium sulfate recovered by hydrometallurgy, wherein the volume ratio of the molar input amount of the sodium carbonate to the lithium-containing waste liquid of the lithium battery is 0.4mol/L, gradually adding 3mol/L sodium hydroxide solution, adjusting the pH value to 11.0 +/-0.2, adding no seed crystal into the waste liquid after the pH value is adjusted, and inducing the nucleation and growth of lithium carbonate crystals in water bath at 50 ℃.
The change of the lithium ion concentration in the waste liquid in example 4 and comparative example 1 was detected by using an inductively coupled plasma emission spectrometer during the crystal deposition, and the result is shown in fig. 2, as the size of the added seed crystal is smaller, the lithium ion concentration in the waste liquid is reduced faster, that is, when the crystallinity is the same, the smaller size seed crystal has stronger promoting effect on the lithium carbonate deposition kinetics, the recovery efficiency of lithium in the waste liquid is higher, the change of the lithium ion concentration in the blank group without the added seed crystal is not obvious, and almost no lithium carbonate crystal is precipitated. That is, when no seed crystal is added to the lithium-containing waste liquid, effective recovery of lithium cannot be achieved. The reason why the lithium content in the blank control group in fig. 2 is reduced is that, as time increases, sodium carbonate added in the lithium-containing waste liquid dissociates carbonate ions and lithium ions are combined, spontaneous nucleation causes formation of a very small amount of lithium carbonate crystals in the solution, but the crystals are further dissolved in the washing process due to too small amount, and cannot be collected, so that the purpose of enriching and recovering lithium cannot be achieved. And after 40 hours, removing the supernatant, adding ethanol to wash the sediment at the bottom, centrifuging to collect the sediment product, and performing vacuum drying at 100 ℃ for 12 hours to obtain a lithium carbonate product, wherein the shape of the lithium carbonate product is shown in the attached figure 3, and D is a lithium carbonate crystal seed addition group, namely the product obtained by the small-size crystal seed addition group is tightly stacked and regular in shape.
Example 5
Adding sodium carbonate into lithium battery waste liquid with the concentration of 0.02mol/L of lithium sulfate recovered by hydrometallurgy, gradually adding 0.1mol/L of sodium hydroxide solution with the volume ratio of the molar input amount of the sodium carbonate to the lithium-containing waste liquid of the lithium battery being 0.02mol/L, adjusting the pH value to 11.0 +/-0.2, adding D lithium carbonate seed crystal into the adjusted waste liquid, the volume ratio of the added mol input amount of the lithium carbonate crystal seed to the lithium-containing waste liquid of the lithium battery is 0.0001mol/L, inducing nucleation and growth of lithium carbonate crystals in a water bath at 25 ℃, removing supernatant after 12.5 hours, adding ethanol to wash bottom sediment, centrifugally collecting sediment products, drying in vacuum at 20 ℃ for 24 hours to successfully obtain a lithium carbonate product, namely, under the condition that the supersaturation degree of the lithium carbonate is far lower than the supersaturation degree of the lithium carbonate, the small-size seed crystal can also induce the deposition of lithium carbonate crystals, and the recovery of lithium in the lithium-containing waste liquid is realized.
Preparing lithium carbonate crystal seeds with same size and different crystallinity
Example 6
3 kinds of nano crystal seeds with different crystallinity are prepared by a dissolution reaction crystallization method: 400mM Na in 100mL2CO3And 400mM Li2SO4Adding 100mL of an anti-solvent DMSO into the mixed solution, adjusting the pH value of the system to be 11, collecting crystallized products of the elution reaction, and washing the crystallized products for 3 times, 4 times and 5 times respectively by using water to obtain seed crystals E, F and G (the crystallinity is respectively 20%, 35% and 100%), wherein the particle size distribution ranges of the seed crystals are 174.04 +/-48.01 nm; 178.16 +/-32.13 nm; 176.94 + -54.45 nm, the lithium carbonate crystal seeds with different crystallinity have the appearance shown in figure 5, figure 4 is the X-ray diffraction pattern (XRD) of the crystal seeds with three different crystallinity, and comparing the (110) peak of the three crystal seeds, the peak width of the crystal seed E is the narrowest, so the crystallinity is the highest, and the peak width of the crystal seed G is the widest, so the crystallinity is the lowest.
Example 7
Adding sodium carbonate into lithium battery waste liquid with the concentration of 0.4mol/L of lithium sulfate recovered by hydrometallurgy, wherein the molar input amount of the sodium carbonate and the volume ratio of the lithium-containing waste liquid of the lithium battery are 0.4mol/L, gradually adding 3mol/L of sodium hydroxide solution, adjusting the pH value to 11.0 +/-0.2, dividing the waste liquid with the adjusted pH value into 3 equal parts, respectively adding E, F, G lithium carbonate crystal seeds prepared by the embodiment 6 into the adjusted waste liquid, wherein the molar input amount of the added lithium carbonate crystal seeds and the volume ratio of the lithium-containing waste liquid of the lithium battery are 0.0005mol/L, inducing nucleation and growth of lithium carbonate crystals in a water bath at 50 ℃, detecting the concentration change of lithium ions in the waste liquid by adopting an inductance coupling plasma emission spectrometer during the crystal deposition, and as shown in figure 6, the higher the crystallinity of the added crystal seeds, the faster the concentration reduction of the lithium ions in the waste liquid, namely, the crystal seeds with the higher crystallinity have the same size and have stronger promotion effect on the lithium carbonate deposition kinetics, the recovery efficiency of lithium in the waste liquid is higher, after 40 hours, the supernatant is removed, ethanol is added to wash the bottom precipitate, the precipitate product is collected by centrifugation and dried in vacuum at 100 ℃ for 12 hours, the lithium carbonate product is obtained, the appearance of the lithium carbonate product is shown in the attached figure 7, and the products obtained by the crystal seed adding groups with different crystallinities are all tightly stacked and have regular appearance.
Claims (7)
1. The application of the lithium carbonate seed crystal in the hydrometallurgical recovery of lithium in the battery is characterized by comprising the following specific implementation processes: adding a certain amount of sodium carbonate into lithium-containing waste liquid of a lithium battery recovered through hydrometallurgy, gradually adding a sodium hydroxide solution or a hydrochloric acid solution to adjust the pH value of the waste liquid to 11.0 +/-0.2, adding a certain amount of lithium carbonate seed crystal into the waste liquid after the pH is adjusted, inducing nucleation and growth of lithium carbonate crystals in a water bath at 25-50 ℃, removing a supernatant after 12.5-40 hours, adding ethanol to wash a bottom precipitate, centrifugally collecting a precipitate product, performing vacuum drying, and finally recovering the lithium carbonate product to achieve the purpose of recovering lithium in the lithium-containing waste liquid.
2. The use of lithium carbonate seed crystal in a hydrometallurgical recovery battery of lithium according to claim 1, wherein the concentration of lithium sulfate in the lithium-containing waste liquid of the lithium battery is 0.02-0.4 mol/L, and the volume ratio of the molar input amount of sodium carbonate to the lithium-containing waste liquid of the lithium battery is 0.02-0.4 mol/L.
3. The use of lithium carbonate seed crystals in hydrometallurgical recovery of lithium from batteries according to claim 1, characterised in that the concentration of the sodium hydroxide solution or hydrochloric acid solution is 0.01 to 3 mol/L.
4. The use of lithium carbonate seed crystals in the hydrometallurgical recovery of lithium from batteries according to claim 1, wherein the ratio of the molar input of lithium carbonate seed crystals to the volume of lithium-containing waste liquid from lithium batteries is 0.0001 to 0.0005 mol/L.
5. Use of lithium carbonate seeds as claimed in claim 1 or 4 for the hydrometallurgical recovery of lithium from batteries, characterized in that the lithium carbonate seeds have a diameter distribution in the range of 190nm to 6 μm and the crystallinity of the lithium carbonate crystals is between 20% and 100%.
6. The use of lithium carbonate seed crystals in hydrometallurgical recovery of lithium from batteries according to claim 5, characterised in that said seed crystals induce nucleation and growth of lithium carbonate crystals for a period of from 12.5 to 24 hours.
7. The application of the lithium carbonate seed crystal in the hydrometallurgical recovery of lithium in the battery according to claim 1, characterized in that ethanol is added to wash bottom precipitates, and the precipitated product obtained after centrifugation is dried in a vacuum drying oven at 20-100 ℃ for 12-24 hours.
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| JP2020132503A (en) * | 2019-02-25 | 2020-08-31 | 住友金属鉱山株式会社 | Purification method of lithium carbonate |
| WO2020196675A1 (en) * | 2019-03-27 | 2020-10-01 | Ｊｘ金属株式会社 | Method for crystallizing carbonate and method for purifying carbonate |
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| JP2020132503A (en) * | 2019-02-25 | 2020-08-31 | 住友金属鉱山株式会社 | Purification method of lithium carbonate |
| WO2020196675A1 (en) * | 2019-03-27 | 2020-10-01 | Ｊｘ金属株式会社 | Method for crystallizing carbonate and method for purifying carbonate |
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